FMOC-Cl柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量

Determination of disodium pamidronate for injection by HPLCpre-column derivatization with FMOC-Cl

目的:建立氯甲酸-9-芴甲酯(FMOC-Cl)柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量。方法:碱性条件下供试品与FMOC-Cl进行衍生化反应,采用Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-0.4%EDTA溶液(用1 mol·L-1氢氧化钠溶液调节pH至7.2)(25∶75),流速1 mL·min-1,检测波长为265 nm。结果:帕米膦酸二钠浓度在0.05～1.00 mg·mL-1范围内与峰面积呈良好关系(r=0.9998),平均回收率为101.0%(n=9)。结论:该方法专属性好,适合用于注射用帕米膦酸二钠的含量测定。

Objective：To develop an HPLC method with pre-column derivatization for the determination of disodium pamidronate for injection.Methods：Disodium pamidronate was derivatized with 9-fluorenylmethyl chloroformate（FMOC-Cl） in 0.05 mol·L-1 Na2CO3 solution,the analytical column was Hypersil ODS2（4.6 mm×250 mm,5 μm） column.The mobile phase consisted of acetonitrile-0.4% EDTA（pH adjusted to 7.2 with 1 mol·L-1 sodium hydroxide solution）（25∶75） at the flow rate of 1.0 mL·min-1,and the detection wavelength was 265 nm.Results：The linear range was 0.05-1.00 mg·mL-1（r=0.9998）,and the average recovery was 101.0%（n=9）.Conclusion：The method is specific and can be used for determination of disodium pamidronate for injection.